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Diethyl Ether → Benzoic acid 2-fluoro-pyridin-4-ylmethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Sodium Benzoate | HCID 517055 | — |
| 反応物 | 4-Bromomethyl-2-fluoropyridine | HCID 13985168 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Benzoic acid 2-fluoro-pyridin-4-ylmethyl ester | HCID 59184859 | 79.4% |
反応手順
The mixture of 4-Bromomethyl-2-fluoro-pyridine (35) (4.85 g, 25.5 mmol) and sodium benzoate (5.51 g, 38.25 mmol) in DMF (60 ml) was stirred at room temperature for 3 hr. Ether was then added and the mixture was washed with water, dried with anhydrous magnesium sulfate, filtered, and evaporated in vacuo. The residue was purified by silica gel column chromatography (eluent, ether:hexane (1:4)) to afford 4.68 g (79%) of a colorless oil; 1H NMR (200 MHz, CDCl3) δ: 5.41 (2H, s), 7.11 (1H, m), 7.45-7.66 (3H, m), 8.08-8.12 (2H, m), 8.23 (1H, d, J=5.4 Hz); m/z (EI): 231 (M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08106064B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-11432487aa5446ddbfa3e0ab506a8082 |
| 出典メモ | uspto-grants-2012_01 |